CN105220205B - A kind of method that composite electrodeposition prepares CNTs/Ni composites - Google Patents
A kind of method that composite electrodeposition prepares CNTs/Ni composites Download PDFInfo
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Abstract
A kind of method that composite electrodeposition prepares CNTs/Ni composites, the present invention relates to the method for preparing composite using composite electrodeposition.In the composite prepared the invention solves prior art the problem of CNT bad dispersibility.Method：First, acid treatment is mixed；2nd, pH value is adjusted；Three~tetra-, it is filtered by vacuum；5th, composite electrodeposition.The present invention uses composite electrodeposition method, can obtain CNT and is uniformly dispersed in metallic matrix, without the good composite of interfacial reaction, interface bond strength.The present invention is used to prepare CNTs/Ni composites.
Description
Technical field
The present invention relates to the method for preparing composite using composite electrodeposition.
Background technology
CNT has excellent mechanical performance, electrical property, magnetic property, optical property and hot property, special at some
Field (such as universe exploration), it is desirable to which high-performance, lightweight, high strength structure material, carbon nano-tube reinforced metal composite has should
Use potentiality.Therefore CNT is considered as a kind of preferable composite material reinforcement body.But CNT is in metallic matrix
Dispersiveness, directly affect with the interfacial reaction of metallic matrix and interface fine structure the performance of composite.Due to carbon nanometer
The specific surface area of pipe is big, and inter-adhesive tangled mass gathers easily in the presence of Van der Waals force, and scattered CNT is once sent out
Raw secondary agglomeration, it is difficult to scatter again.This aggregate can make CNT lose its invigoration effect in the composite.Separately
Outer CNT and some metals, such as aluminium alloy, easily occur interfacial reaction at high temperature.Last CNT and Metal Substrate
Body forms good physics, chemical interface intensity, the good physical and mechanical properties of competence exertion CNT.
The content of the invention
In the composite prepared the invention solves prior art the problem of CNT bad dispersibility, and provide a kind of
The method that composite electrodeposition prepares CNTs/Ni composites.
A kind of method that composite electrodeposition prepares CNTs/Ni composites, is specifically followed the steps below：
First, carbon nanotube dust is mixed with concentrated nitric acid, adds the concentrated sulfuric acid, then under mechanical agitation, carried out
Intermittence is ultrasonically treated 25h, is 30min per ultrasonic time, intermittent time 2h, obtains suspension；Wherein carbon nanotube dust
For 15g, concentrated nitric acid volume is 250mL, concentrated sulfuric acid volume 750mL；
2nd, in the suspension for obtaining distilled water addition step 1, it is 2000mL to volume, stirs, then stand
Sediment is produced, when the volume of sediment reaches 1000mL, topples over upper solution；Repeat operation：Distilled water is added to body
Product is 2000mL, is stirred, and then stands and produces sediment, when the volume of sediment reaches 1000mL, it is molten to topple over upper strata
Liquid；When pH to upper solution is 1.8~2.1, retains upper solution, obtain solidliquid mixture；
3rd, step 2 is obtained into solidliquid mixture to pour into Buchner funnel, be filtered by vacuum, filtered film and filtered using micropore
Film；When liquid level is less than cloth one half height of funnel, distilled water diluting is toppled over, be 6~7 to the pH value for filtering out liquid, stop
Only topple over distilled water, complete to filter, obtain powder；
4th, the powder for obtaining step 3 is well mixed with solvent, is then filtered by vacuum, and is filtered sieve and is used 800 mesh
Brass wire cloth, the product of sieving is filtered by vacuum again, filters film and use miillpore filter, obtain CNT；
5th, the CNT that nickel sulfate, nickel chloride, boric acid and step 4 obtain is well mixed, ultrasonic disperse 30min,
Electrolyte is configured to, then carries out composite electrodeposition, wherein control composite electrodeposition technological parameter：Temperature is 50 DEG C, and magnetic force stirs
Mix speed 100rpm, electrolyte ph 4.0, cathode-current density 1A/dm2, electrodeposition time 2h, it is compound to obtain CNTs/Ni
Material.
The beneficial effects of the invention are as follows：
Composite electrodeposition is a kind of new composite technology of preparing in the present invention.More other preparation methods, such as
Powder metallurgy, Pressure Infiltration, stirring casting, hot extrusion, composite electrodeposition have following features：
1st, preparation temperature is low.Composite electrodeposition is carried out in the aqueous solution or organic solvent, and typical temperature is controlled at 50 DEG C
~70 DEG C；Traditional handicraft temperature is typically larger than 500 DEG C.
2nd, good economy performance.On the basis of conventional electrodeposition device, electrolyte, anode, being subject to applicability transformation can enter
Row composite electrodeposition, therefore less investment, expense is low, energy consumption is small.
3rd, it is easily controlled.Composite electrodeposition is easy to operate, easily controllable.
4th, applicability is wide.The reinforcement particulate that one or more sizes are different, distinct can be added in electrolyte, together
Kind particulate can also be added in different electro-deposition systems, in embedded different-alloy matrix or elemental metals matrix, can be prepared not
Congener composite.
The present invention is used to prepare CNTs/Ni composites.
Brief description of the drawings
Fig. 1 is that the step 3 of embodiment one and step 4 are illustrated using miillpore filter as Vacuum filtration device when filtering film
Figure, wherein 1 represents miillpore filter, 2 represent mechanical agitation rod, and 3 represent plastic funnel, and 4 represent Buchner funnel, and 5 represent round bottom burning
Bottle, 6 represent rubber tube, and 7 represent vavuum pump；
Fig. 2 is that the step 4 of embodiment one is used as Vacuum filtration device schematic diagram when filtering film using brass wire cloth, wherein 4 represent
Buchner funnel, 5 represent round-bottomed flask, and 6 represent rubber tube, and 7 represent vavuum pump, and 8 represent brass wire cloth；
Fig. 3 is the schematic device that the step 5 of embodiment one carries out composite electrodeposition, wherein 9 represent electrode fixed station, 10
Represent anode nickel sheet, 11 represent plating piece, and 12 represent magnetic agitation rotor, and 13 represent constant temperature blender with magnetic force, and 14 to represent direct current steady
Voltage source；
Fig. 4 is the CNTs stereoscan photographs that the step 4 of embodiment one sieves to obtain；
Fig. 5 is the metallograph in CNTs/Ni composite sheets section prepared by embodiment one；
Fig. 6 and Fig. 7 is that the surface scan Electronic Speculum of CNTs/Ni composites prepared by embodiment one is shone, and wherein Fig. 6 is low
Times, Fig. 7 is high power；
Fig. 8 is the X-ray diffraction spectrogram of CNTs/Ni composites prepared by embodiment one；
Fig. 9 is the extension test curve map of CNTs/Ni composites prepared by one~example IV of embodiment.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：The method that a kind of composite electrodeposition of present embodiment prepares CNTs/Ni composites, specifically
Follow the steps below：
First, carbon nanotube dust is mixed with concentrated nitric acid, adds the concentrated sulfuric acid, then under mechanical agitation, carried out
Intermittence is ultrasonically treated 25h, is 30min per ultrasonic time, intermittent time 2h, obtains suspension；Wherein carbon nanotube dust
For 15g, concentrated nitric acid volume is 250mL, concentrated sulfuric acid volume 750mL；
2nd, in the suspension for obtaining distilled water addition step 1, it is 2000mL to volume, stirs, then stand
Sediment is produced, when the volume of sediment reaches 1000mL, topples over upper solution；Repeat operation：Distilled water is added to body
Product is 2000mL, is stirred, and then stands and produces sediment, when the volume of sediment reaches 1000mL, it is molten to topple over upper strata
Liquid；When pH to upper solution is 1.8~2.1, retains upper solution, obtain solidliquid mixture；
3rd, step 2 is obtained into solidliquid mixture to pour into Buchner funnel, be filtered by vacuum, filtered film and filtered using micropore
Film；When liquid level is less than cloth one half height of funnel, distilled water diluting is toppled over, be 6~7 to the pH value for filtering out liquid, stop
Only topple over distilled water, complete to filter, obtain powder；
4th, the powder for obtaining step 3 is well mixed with solvent, is then filtered by vacuum, and is filtered sieve and is used 800 mesh
Brass wire cloth, the product of sieving is filtered by vacuum again, filters film and use miillpore filter, obtain CNT；
5th, the CNT that nickel sulfate, nickel chloride, boric acid and step 4 obtain is well mixed, ultrasonic disperse 30min,
Electrolyte is configured to, then carries out composite electrodeposition, wherein control composite electrodeposition technological parameter：Temperature is 50 DEG C, and magnetic force stirs
Mix speed 100rpm, electrolyte ph 4.0, cathode-current density 1A/dm2, electrodeposition time 2h, it is compound to obtain CNTs/Ni
Material.
Embodiment two：Present embodiment is unlike embodiment one：Concentrated nitric acid quality in step 1
Concentration is 69%.It is other identical with embodiment one.
Embodiment three：Present embodiment is unlike embodiment one or two：The concentrated sulfuric acid in step 1
Mass concentration is 98%.It is other identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Surpass in step 1
Acoustic treatment frequency is 40kHz.It is other identical with one of embodiment one to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：It is molten in step 4
Agent is distilled water or absolute ethyl alcohol.It is other identical with one of embodiment one to four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：Step 5 is electrolysed
Concentration of nickel sulfate is 240g/L in liquid.It is other identical with one of embodiment one to five.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：Step 5 is electrolysed
Chlorination nickel concentration is 40g/L in liquid.It is other identical with one of embodiment one to six.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：Step 5 is electrolysed
Liquid mesoboric acid concentration is 40g/L.It is other identical with one of embodiment one to seven.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：Step 5 is electrolysed
Carbon nanotube concentration is 0.5~1.25g/L in liquid.It is other identical with one of embodiment one to eight.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：Step 5 is compound
Electro-deposition anode uses nickel sheet.It is other identical with one of embodiment one to nine.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
The method that a kind of composite electrodeposition of the present embodiment prepares CNTs/Ni composites, specifically enters according to following steps
Capable：
First, carbon nanotube dust is mixed with concentrated nitric acid, adds the concentrated sulfuric acid, then under mechanical agitation, carried out
Intermittence is ultrasonically treated 25h, is 30min per ultrasonic time, intermittent time 2h, obtains suspension；Wherein carbon nanotube dust
For 15g, concentrated nitric acid volume is 250mL, concentrated sulfuric acid volume 750mL；Concentrated nitric acid mass concentration is 69%, concentrated sulfuric acid mass concentration
For 98%；Supersound process frequency is 40kHz；
2nd, in the suspension for obtaining distilled water addition step 1, it is 2000mL to volume, stirs, then stand
Sediment is produced, when the volume of sediment reaches 1000mL, topples over upper solution；Repeat operation：Distilled water is added to body
Product is 2000mL, is stirred, and then stands and produces sediment, when the volume of sediment reaches 1000mL, it is molten to topple over upper strata
Liquid；When pH to upper solution is 1.8~2.1, retains upper solution, obtain solidliquid mixture；
3rd, step 2 is obtained into solidliquid mixture to pour into Buchner funnel, be filtered by vacuum, filtered film and filtered using micropore
Film；When liquid level is less than cloth one half height of funnel, distilled water diluting is toppled over, be 6~7 to the pH value for filtering out liquid, stop
Only topple over distilled water, complete to filter, obtain powder；
4th, the powder for obtaining step 3 is well mixed with solvent, is then filtered by vacuum, and is filtered sieve and is used 800 mesh
Brass wire cloth, the product of sieving is filtered by vacuum again, filters film and use miillpore filter, obtain CNT；Solvent is anhydrous
Ethanol；
5th, the CNT that nickel sulfate, nickel chloride, boric acid and step 4 obtain is well mixed, ultrasonic disperse 30min,
Electrolyte is configured to, then carries out composite electrodeposition, wherein control composite electrodeposition technological parameter：Temperature is 50 DEG C, and magnetic force stirs
Mix speed 100rpm, electrolyte ph 4.0, cathode-current density 1A/dm2, electrodeposition time 2h, it is compound to obtain CNTs/Ni
Material；
Wherein, concentration of nickel sulfate is 240g/L in electrolyte, and chlorination nickel concentration is 40g/L, boric acid concentration 40g/L, carbon
Concentrations of nanotubes is 1.0g/L, and anode uses nickel sheet.
The present embodiment step 3 and step 4 using miillpore filter as Vacuum filtration device when filtering film as shown in figure 1,
Wherein 1 represents miillpore filter, and 2 represent mechanical agitation rod, and 3 represent plastic funnel, and 4 represent Buchner funnel, and 5 represent round-bottomed flask, and 6
Rubber tube is represented, 7 represent vavuum pump.
The present embodiment step 4 is using brass wire cloth as Vacuum filtration device when filtering film as shown in Fig. 2 wherein 4 represent cloth
Family name's funnel, 5 represent round-bottomed flask, and 6 represent rubber tube, and 7 represent vavuum pump, and 8 represent brass wire cloth.
The present embodiment step 5 carries out the installation drawing of composite electrodeposition as shown in figure 3, wherein 9 represent electrode fixed station, and 10
Represent anode nickel sheet, 11 represent plating piece, and 12 represent magnetic agitation rotor, and 13 represent constant temperature blender with magnetic force, and 14 to represent direct current steady
Voltage source.
The CNTs stereoscan photographs that the present embodiment step 4 sieves to obtain are as shown in figure 4, as can be seen from the figure carbon is received
Mitron is in dispersity, does not form reunion.
The metallograph in CNTs/Ni composite sheets section manufactured in the present embodiment as described in Figure 5, as seen from the figure
Composite material sheet layer thickness homogeneity is preferable, does not observe that big cavity and CNTs reunite.
The surface scan electromicroscopic photograph of CNTs/Ni composites manufactured in the present embodiment as shown in Figure 6 and Figure 7, wherein Fig. 6
For low power, Fig. 7 is high power；
A is that CNT one end is embedded in film in Fig. 6, and the other end is suspended in electrolyte, and deposited the shape of nickle atom
State, linear part are stuck in film surface；B is that CNT both ends are embedded in film, and center section, which exposes, to be come and be suspended in
In electrolyte, exposed part deposited nickle atom, form the form of bridge like.Observation carbon nano tube surface can see its section
Shape feature, this is wrapped CNT by some nickel balls and is contacted with each other and form；
The CNT of nickel is deposited by being observed that in Fig. 7 high power stereoscan photographs, as arrow a is signified.Carbon is received
During mitron both ends are embedded into film only, interlude is exposed outside and be in suspended state, and nickle atom deposits to the carbon of this state
On nanotube, hanging bridge shape pattern is formd, the nickel for being wrapped in CNT is in nodular form.Observing picture surface can be with
See thread material, should be CNT.Thread CNT is fitted in the surface of film.
X-ray diffraction spectrogram such as Fig. 8 of CNTs/Ni composites manufactured in the present embodiment, due to the carbon in composite
Content is too low, and X-ray diffraction can not detect micro carbon, therefore can't see the diffraction maximum of carbon.It can be seen by Fig. 8
Go out three main diffraction maximums of nickel dam.
Embodiment two：
The method that a kind of composite electrodeposition of the present embodiment prepares CNTs/Ni composites, specifically enters according to following steps
Capable：
First, carbon nanotube dust is mixed with concentrated nitric acid, adds the concentrated sulfuric acid, then under mechanical agitation, carried out
Intermittence is ultrasonically treated 25h, is 30min per ultrasonic time, intermittent time 2h, obtains suspension；Wherein carbon nanotube dust
For 15g, concentrated nitric acid volume is 250mL, concentrated sulfuric acid volume 750mL；Concentrated nitric acid mass concentration is 69%, concentrated sulfuric acid mass concentration
For 98%；Supersound process frequency is 40kHz；
2nd, in the suspension for obtaining distilled water addition step 1, it is 2000mL to volume, stirs, then stand
Sediment is produced, when the volume of sediment reaches 1000mL, topples over upper solution；Repeat operation：Distilled water is added to body
Product is 2000mL, is stirred, and then stands and produces sediment, when the volume of sediment reaches 1000mL, it is molten to topple over upper strata
Liquid；When pH to upper solution is 1.8~2.1, retains upper solution, obtain solidliquid mixture；
3rd, step 2 is obtained into solidliquid mixture to pour into Buchner funnel, be filtered by vacuum, filtered film and filtered using micropore
Film；When liquid level is less than cloth one half height of funnel, distilled water diluting is toppled over, be 6~7 to the pH value for filtering out liquid, stop
Only topple over distilled water, complete to filter, obtain powder；
4th, the powder for obtaining step 3 is well mixed with solvent, is then filtered by vacuum, and is filtered sieve and is used 800 mesh
Brass wire cloth, the product of sieving is filtered by vacuum again, filters film and use miillpore filter, obtain CNT；Solvent is anhydrous
Ethanol；
5th, the CNT that nickel sulfate, nickel chloride, boric acid and step 4 obtain is well mixed, ultrasonic disperse 30min,
Electrolyte is configured to, then carries out composite electrodeposition, wherein control composite electrodeposition technological parameter：Temperature is 50 DEG C, and magnetic force stirs
Mix speed 100rpm, electrolyte ph 4.0, cathode-current density 1A/dm2, electrodeposition time 2h, it is compound to obtain CNTs/Ni
Material；
Wherein, concentration of nickel sulfate is 240g/L in electrolyte, and chlorination nickel concentration is 40g/L, boric acid concentration 40g/L, carbon
Concentrations of nanotubes is 0.5g/L, and anode uses nickel sheet.
Embodiment three：
The method that a kind of composite electrodeposition of the present embodiment prepares CNTs/Ni composites, specifically enters according to following steps
Capable：
First, carbon nanotube dust is mixed with concentrated nitric acid, adds the concentrated sulfuric acid, then under mechanical agitation, carried out
Intermittence is ultrasonically treated 25h, is 30min per ultrasonic time, intermittent time 2h, obtains suspension；Wherein carbon nanotube dust
For 15g, concentrated nitric acid volume is 250mL, concentrated sulfuric acid volume 750mL；Concentrated nitric acid mass concentration is 69%, concentrated sulfuric acid mass concentration
For 98%；Supersound process frequency is 40kHz；
2nd, in the suspension for obtaining distilled water addition step 1, it is 2000mL to volume, stirs, then stand
Sediment is produced, when the volume of sediment reaches 1000mL, topples over upper solution；Repeat operation：Distilled water is added to body
Product is 2000mL, is stirred, and then stands and produces sediment, when the volume of sediment reaches 1000mL, it is molten to topple over upper strata
Liquid；When pH to upper solution is 1.8~2.1, retains upper solution, obtain solidliquid mixture；
3rd, step 2 is obtained into solidliquid mixture to pour into Buchner funnel, be filtered by vacuum, filtered film and filtered using micropore
Film；When liquid level is less than cloth one half height of funnel, distilled water diluting is toppled over, be 6~7 to the pH value for filtering out liquid, stop
Only topple over distilled water, complete to filter, obtain powder；
4th, the powder for obtaining step 3 is well mixed with solvent, is then filtered by vacuum, and is filtered sieve and is used 800 mesh
Brass wire cloth, the product of sieving is filtered by vacuum again, filters film and use miillpore filter, obtain CNT；Solvent is anhydrous
Ethanol；
5th, the CNT that nickel sulfate, nickel chloride, boric acid and step 4 obtain is well mixed, ultrasonic disperse 30min,
Electrolyte is configured to, then carries out composite electrodeposition, wherein control composite electrodeposition technological parameter：Temperature is 50 DEG C, and magnetic force stirs
Mix speed 100rpm, electrolyte ph 4.0, cathode-current density 1A/dm2, electrodeposition time 2h, it is compound to obtain CNTs/Ni
Material；
Wherein, concentration of nickel sulfate is 240g/L in electrolyte, and chlorination nickel concentration is 40g/L, boric acid concentration 40g/L, carbon
Concentrations of nanotubes is 0.75g/L, and anode uses nickel sheet.
Example IV：The method that a kind of composite electrodeposition of the present embodiment prepares CNTs/Ni composites, specifically according to
What lower step was carried out：
First, carbon nanotube dust is mixed with concentrated nitric acid, adds the concentrated sulfuric acid, then under mechanical agitation, carried out
Intermittence is ultrasonically treated 25h, is 30min per ultrasonic time, intermittent time 2h, obtains suspension；Wherein carbon nanotube dust
For 15g, concentrated nitric acid volume is 250mL, concentrated sulfuric acid volume 750mL；Concentrated nitric acid mass concentration is 69%, concentrated sulfuric acid mass concentration
For 98%；Supersound process frequency is 40kHz；
2nd, in the suspension for obtaining distilled water addition step 1, it is 2000mL to volume, stirs, then stand
Sediment is produced, when the volume of sediment reaches 1000mL, topples over upper solution；Repeat operation：Distilled water is added to body
Product is 2000mL, is stirred, and then stands and produces sediment, when the volume of sediment reaches 1000mL, it is molten to topple over upper strata
Liquid；When pH to upper solution is 1.8~2.1, retains upper solution, obtain solidliquid mixture；
3rd, step 2 is obtained into solidliquid mixture to pour into Buchner funnel, be filtered by vacuum, filtered film and filtered using micropore
Film；When liquid level is less than cloth one half height of funnel, distilled water diluting is toppled over, be 6~7 to the pH value for filtering out liquid, stop
Only topple over distilled water, complete to filter, obtain powder；
4th, the powder for obtaining step 3 is well mixed with solvent, is then filtered by vacuum, and is filtered sieve and is used 800 mesh
Brass wire cloth, the product of sieving is filtered by vacuum again, filters film and use miillpore filter, obtain CNT；Solvent is anhydrous
Ethanol；
5th, the CNT that nickel sulfate, nickel chloride, boric acid and step 4 obtain is well mixed, ultrasonic disperse 30min,
Electrolyte is configured to, then carries out composite electrodeposition, wherein control composite electrodeposition technological parameter：Temperature is 50 DEG C, and magnetic force stirs
Mix speed 100rpm, electrolyte ph 4.0, cathode-current density 1A/dm2, electrodeposition time 2h, it is compound to obtain CNTs/Ni
Material；
Wherein, concentration of nickel sulfate is 240g/L in electrolyte, and chlorination nickel concentration is 40g/L, boric acid concentration 40g/L, carbon
Concentrations of nanotubes is 1.25g/L, and anode uses nickel sheet.
One~example IV of embodiment prepare CNTs/Ni composites extension test curve map as shown in figure 9, its
In, ☆ represents embodiment one, and represents embodiment two, ▲ embodiment three is represented, * represents example IV, it can be seen that THIN COMPOSITE
Film elongation percentage is smaller, less than 1.0%.From stress-strain diagram it can be seen that laminated film plastic period in drawing process
Unobvious.There is peak value in 0.75g/L in tensile strength.
Claims (3)
1. a kind of method that composite electrodeposition prepares CNTs/Ni composites, it is characterised in that this method is specifically according to following
What step was carried out：
First, carbon nanotube dust is mixed with concentrated nitric acid, adds the concentrated sulfuric acid, then under mechanical agitation, carry out interval
Property be ultrasonically treated 25h, per ultrasonic time be 30min, intermittent time 2h, obtain suspension；Wherein carbon nanotube dust is
15g, concentrated nitric acid volume are 250mL, concentrated sulfuric acid volume 750mL；
2nd, in the suspension for obtaining distilled water addition step 1, it is 2000mL to volume, stirs, then stands and produce
Sediment, when the volume of sediment reaches 1000mL, topple over upper solution；Repeat operation：Adding distilled water to volume is
2000mL, stir, then stand and produce sediment, when the volume of sediment reaches 1000mL, topple over upper solution；Extremely
When the pH of upper solution is 1.8~2.1, retains upper solution, obtain solidliquid mixture；
3rd, step 2 is obtained into solidliquid mixture to pour into Buchner funnel, be filtered by vacuum, filtered film and use miillpore filter；
When liquid level is less than cloth one half height of funnel, distilled water diluting is toppled over, be 6~7 to the pH value for filtering out liquid, stop inclining
Distilled water, complete to filter, obtain powder；
4th, the powder for obtaining step 3 is well mixed with solvent, is then filtered by vacuum, and is filtered sieve and is used 800 mesh copper mesh
Sieve, the product of sieving is filtered by vacuum again, is filtered film and is used miillpore filter, obtains CNT；
5th, the CNT that nickel sulfate, nickel chloride, boric acid and step 4 obtain is well mixed, ultrasonic disperse 30min, prepared
Into electrolyte, composite electrodeposition is then carried out, wherein control composite electrodeposition technological parameter：Temperature is 50 DEG C, magnetic agitation speed
Rate 100rpm, electrolyte ph 4.0, cathode-current density 1A/dm2, electrodeposition time 2h, obtain CNTs/Ni composites；
It is 40kHz that frequency is ultrasonically treated in step 1；Solvent is absolute ethyl alcohol in step 4；
Wherein, concentration of nickel sulfate is 240g/L in electrolyte, and chlorination nickel concentration is 40g/L, boric acid concentration 40g/L, carbon nanometer
Pipe concentration is 0.75g/L, and anode uses nickel sheet.
2. the method that a kind of composite electrodeposition according to claim 1 prepares CNTs/Ni composites, it is characterised in that step
Concentrated nitric acid mass concentration is 69% in rapid one.
3. the method that a kind of composite electrodeposition according to claim 1 prepares CNTs/Ni composites, it is characterised in that step
Concentrated sulfuric acid mass concentration is 98% in rapid one.
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| CN106591926B (en) * | 2016-12-09 | 2018-10-02 | 济南大学 | In the method that steel surface prepares the porous nickel nickel evolving hydrogen reaction catalyst of CNTs- |
| CN106521550B (en) * | 2016-12-09 | 2018-09-25 | 济南大学 | Nickel foam/LBL self-assembly carbon nanotube/nickel composite material preparation method for electrolytic hydrogen production |
| CN106680418A (en) * | 2016-12-29 | 2017-05-17 | 武汉大学 | Method for detecting content of enhanced material in metal-based carbon composite nano-material |
| CN108034984A (en) * | 2017-12-07 | 2018-05-15 | 哈尔滨工业大学 | A kind of preparation method of carbon nanotubes copper-based laminated composite material |
| CN108570697A (en) * | 2018-04-26 | 2018-09-25 | 大同新成新材料股份有限公司 | A kind of Brush Plating composite technology |
| CN110512245A (en) * | 2019-09-19 | 2019-11-29 | 昆明理工大学 | A method of improving composite material corrosive nature |
| CN111020656A (en) * | 2019-11-06 | 2020-04-17 | 昆明理工大学 | Method for improving friction and wear performance of composite material |
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